Process of making cellulose



B; LOOMIS. PROCESS or MAKING CELLULOSE.

APPLICATION FILEIT NOV- I, I916- 1 .311 ,980. Patented Aug. 5, 191% 2 SHEETSSHEET 1.'

- j WM B. LOOMIS.

PROCESS or MAKING CELLULOSE.

APPLICATION' HLED NOV. I, I916.

- Patented Aug 5, 1919.

2 SHEETS-SHEET 2.

UNITED STATES PATENT OFFICE.

BURDETT LOOMI S, 0F HARTFORD, CONNECTICUT, ASSIGNOR TO GRACE L. LOOMIS, 0F HARTFORD. CONNECTICUT.

PROCESS OF MAKING CELLULOSE.

Specification of Letters Patent.

Patented A ug. 5, 1 919.

To all whom it may concern,

Be it known that l. Birnnl-l'r'r LooMIs, citizen of the United States, residing at Hartford, in the county of Hartford and State of Connecticut. have invented certain new and useful Irmirovements in Processes of Making Cellulose, of which the following is a specification.

This invention relates to the manufacture of cellulose fromvarious kinds of plants and fiber material in the green condition.-

The principal object of my invention is to provide a process for more ellectively and economically'reducing green plant material to cellulose for paper making; also to extract and save natural constituents, such as tannic acid, saccharine matter, gummy and resinous matter, etc. from various kinds of 1 plant. material. A special object is to provide for producing cellulose with stronger and better fiber by thoroughly extracting the saccharine matter from green plant material by macerating the material in water or plant liquor at a. low temperature,-from about 100 F. to 200 F.and then drawing off the liquor and adding fresh water, thereby developing a class of bacteria which do not attack or injure the fiber, but on the contrary leaves it strong and of increased value. The water .or liquor may be drawn ofi and fresh water added'several times] during the treating operation for betterlseparating the different constituents of the lant material.

Another object is .to provide for better comminnting or shiredding plant material and transferring orforcing it to a digester or treating tank, 1 circulating numerous streams of warm water or liquor through the material and through a heater. passingthe pulp material from the digester to a heating engine and forcing the finished cellulose to a paper machine.

other objects and purposes of my inven tion will appear in the following description of the process.

The matter constituting my invention will be set forth. in the claims,

I will now describe my process in. con- ,nection with the accompanying drawings circulating liquid. a cane press 40. a shredder -l-5 and a heating engine 50, all suitably connected by pipcs quunps. etc. The treating tank 2 is constructed of plate iron with a contractwl or drawn in bottom 2, to which is connected a discharge pipe 2" leading to a hentingcnginc 50. The pipe 2" is provided with a gate valve 2, having a stem 2. Within tank 2 is suspended a movable distributing pipe system 3, composed of a sliding telescopic pipe 4, a series of radial and circular pipes 5 and numerous depending discharge pipcs 0, of suitable lengths-to extend to the contracted bottom when in the lowered position, as shown in full lines. The dotted lines indicate that the systeln'may be raised for better (.lischarging the contents of the tank. The radial pi )es are connected by a fitting 1) to pipe 4. lhe fixed liquid supply pipe (attends down through a, stufling box a into pipe 4 and the latter'pipc slides liquor containing extracts, such as tannin or saccharine matter.

BVith the side of tank 2 areconnectcd ou let pipes I l-+40, having valves (l-(l', and connecting with the upright pipes 11 11.. Pipe 11 has a valve rl" and leads to a condenser 12, liming the usual inlet and outlet; pipes for cooling water, and a bottom discharge pipe 13, having a valve a, connecting with a seal box 14 for products of condensation. I

A gas heating coil- 1!) is placed in a casing and has a gas supply pipe 20, having a valve and an outlet pipe '22, having a valve h, connecting with pipe 18. A gas pipe 21, having a valve 7' supplies a burner 21?. A neutral gas composed largely of hydrogen may be heated in the coil and Chains 16 are- The coil 23 is heated by a gas burner 25 having a supply pipe and valve s. A sup ply pipe 26, having a valve t, for milk of lime or alkaline solution, connects with pipe 7 at the T-l'itting '4.

A pipe having a valve m, connects with pipe 11 and with a rotary force pump 31, from which a pipe 32 leads to a heating coil 33 in furnace 34. having a gas burner 35 and supply pipe having a valve 0. An

outlet pipe 56., having a check valve n leads from the coil and connects with pipe 18. The pipe 36 also has a valve 7). A branch pipe 36", having a valve 9 connects pipe 36 with a. liquor storage tank 37, which may he of any desired size.

For the purpose of pressing out juice containingsaccharinematter from cane. Kafir corn stalks and other material I provide pressure rolls 40 mounted in a frame, also a juice pan ll. 11 pipe 42 leads from the pan to a storage tank 43. feeding chute 44c and a discharge chute 44 are secured to the frame, and the chute *l-l connects with a, shredding machine 45. This machine reduces the cane and other plant material to short lengths and comparatively fine shreds,

ready for treatment in the diti'usion and extracting tank 2. A discharge pip ll; connects the case of the shredder with a rotary exhauster and blower 47, having a discharge nozzle 48, with which connects the feed. pipe 8 opening into the treating tank The exhauster and blower operates to draw off the shredded material and discharge it into tank 2.

A l eating engine 50 may connect directly Withthe discharge pipe 2* of tank "2 as shown. and will operate in a well known manner to reduce the shredded and digested material to pulp or cellulose. An outlet pipe 52 may connect the engine with a rotary hauster 53 having a discharge pipe 54:. Ar

pipe 51 having a valve u, connects with the beating engine and may be used for supplying-a bleaching solution or liquor,'si1ch as hypochlorite of sodium. or chlorid of lime. The pipe 54 may connect ,with a storage tank or directly to a paper making machine.

In carrying out my process I treat green plants. such as marsh grass, rushes, palmetto, Kafir corn, sugar cane, sunflower stalks, banana stalks, etc, and first press out. the juice which contains a valuable per cent. of saccharine matter.

This juice is' saved and may be fermented in a well known manner and the mash distilled for recovering the alcohol. The juice may also be concentrated for producing a syrup suitable for I body of material. The water will pass uniformly up throughthe shredded material and extract the saccharine n-iatter. An even. ten'iperature below 150 F. is n'iaintained for, a period of eight to twelve hours, accoriiling to the kind of plant heing treated. The n'iaterial is thus subjected to a steeping or dittusion operation till the saccharine matter is extracted, then a fermentation process sets iin'tlue to the development of bacteria that feed on the sugar and which. if left in the t-anlt drstroy the value of the plant fiber. At this stage I therefore draw oil the liquor through pipe 9 and admit fresh water and continue the treatment. Another class of bacteria now developed which do not attack or injure the fiber. If it is desired particularly to obtain fiber the temperature iskept low for the necessary length of time to separate the fiber. In cage cellulose or pulp is to he made the temperature may be raised to, or above, 150 F. and the liquor will be circulated by the pump 31 through the heater coil 33, then through pipes 36. 18,

valve 2" into the beating engine 50 where it is 'ircpared for the paper making machine.

In the beater engine I preferably add-chlorid of lime or hypochlorites, solution through pipe 51.

A Warm neutral gas, such as Water-gas or producer gas, may be passed into the digester tank 2 for driving out oxygen and vapors ,of volatile oils. These vapors will be condensed in the conclenser 12 and the oil collected. Gas may also be forced under pressure into the treating tank atthe end of the' extracting or digesting operation to force out the steeped or cooked material through pipe 2?. My process is not confined to passing the treated material directly to the beating engine; it may be discharged into any tank or not as desired.

The operation of driiwing ofi liquor eontaining extracted matter of any kind may by admitting a be repeated with the addition of fresh water to the tank several times, in order to re- 4 move matter not desired in paper pulp or cellulose. In case palmetto plants and roots f are being treated for extracting tannic acid and preparing cellulose, the temperature is preferably maintained for the first period of several hours at about 100 F., and then it is raised to about 150 F. and kept at that degree till extraction is completed. The liquor is then drawn oil: and may be concentrated. While extracting the tannic acid the temperature of the liquor should never be raised to the boiling point as that tem- 'perature injures the properties of the extract and causestoo much of the gummy matter to be dissolved. After the tannin extract has been drawn oil fresh water may be admitted to the tank and the temperature raised to about 212 F. for dissolving part of the gummy matter, and at this stage an alkaline solution may be admitted through pipe 26 for expediting the operation. This is important at this particular stage of the treatment.

By my process of extracting saccharine matter, tannic acid and other constituents,

first at a low temperature of about 100 F., then at about 150 F., much better extractstannic acid, saccharine matter, etc.-are produced, and the fiber of the plant material is made much stronger. By my method of treatment the strength of palmetto fiber has been increasedfifty per cent. This is a very valuable improvement in the art of preparing fiber plant material either for cellulose or for fiber to be made into rope or a woven fabric. The above remarks apply to the banana plant, Kafir corn. sugar cane and other plant material. In my process the liquor is preferably circulated by a pump 31 through a heater and thence in numerous streams through the body of material in tank 2. Part of the liquor is also prefother valuable results.

The treating tank and connections may be of modified construction as shown in Fig. Here the treating tank 2 may be constructed to be heated externally, as by a stove or furnace. Inlet pipes l and 5*. having discharge pipe fi may supply water or liquor in numerous streams close to the flat bottom of the tank. i The water will be spread over the bottom and then rise through the shredded material. A discharge pipe 2 for pulp is connected to the bottom of the tank and hasxa gate valve. A draw-otf pipe 9 for liquor, having a valve 1: may connect with pipe 52 or with other convenient part as shownl A fillingopening 8?, having a cover, is placed in the top of the tank. A liquor and vapor discharge pipe 10". having a valve d leads from the top of the tank and connects with a depositing and separating chamber 55-55, having a (lefiecting hood 56. An outlet pipe 30, having'a valve m, connects below the top of the hood and leads to a circulating pump 31. The discharge pipe 32 of the pump connects with the inlet pipe 4 of the tank 2. An elevated tank 57 is provided for holding an alkaline solution or a bleaching liquor, and connects by a valved pipe 58 with pipe 32. or it may connect in any other manner with, tank 2.

The operation in this mod fied form of apparatus in substantially the .sume as that above described with reference to Fig. 1. Provision. howcv'cr. is here made for separating resinous or gummy matter in the depositing chamber 5555. This is important and valuable when fiber material containing much gummy or resinous matter is being treated. \Vith the connection shown the alkaline solution will be spread uniformly over the bottom of the treating tank and then passed uniformly up through the whole mass of the fiber material.

In practice all the necessary pressure gages and thermometers are placed on the apparatus so as to exactly regulate the heat and pressure as re uired.

Having descrilie my invention, what I claim, and desire to secure by Letters Patent, 1s:

1. The process of making cellulose, which consists in subjecting shredded green plant material to maceratiom in a closed chamber at a temperature below the boiling point and circulating the liquid in streams through the material, then drawing oil' the liquid extract. adding fresh water and an alkaline chemical to the material and raising the temperature to about 212" F. to dissolve gummy and resinous matter and finish the cooking operation, whereby cellulose of strong fiber is produced.

2. The process oi making cellulose, which.

at a temperature below the boiling point and circulating the liquid in streams through the material, then drawing off the liquid extract and circulating fresh water at a gradually increased temperaturethrough the material, adding an alkaline chemical to the material and raising the temperature to about 212 F.

to finish the cooking operation, whereby cellulose of strong fiber is produced.

circulating the liquid in streams through the material for extracting saccharine and other matter, drawing oft liquid extract,

adding and circulating fresh water at an increased temperature, adding alkali and continuingthe cooking-operation till finished, then transferring the cooked 'material to a beating engine and thercinpreparing it for paper making.

5. The process of making cellulose, which consists in inacerating green plant material at a .temperature'of about 100 F. for extracting saccharine and other matter, drawing oftthe liquid. extract and adding fresh water repeatedly .and, maintaining a .tem perature of about 150 F., circulating the liquid in streams through the material and continuing the operation at a low temperature to avoid dissolving the gummy or resinous matter in the material and finally increasing the temperature to finish the cookin g operation.

consists in pressing the juice from plant material, then shredding and disc arg ing it'to a treating tank, then maeerating the material at a tempera ure which Will not dissolvethe gummy matter, drawing off the liquid extract and edding'fresh Water and finishing the treatment at an increased. temperature.

In testimony whereof I affix my signature in presence of two Witnesses.

. BURDETT Looms.

'W'itnesses:

G. L. LOOMIS, LUCRETIA M. Looms.

6. The process of making eellu1ose,'whieh' reen 

